JP2001329173A - Heat-conductive silicone gel composition - Google Patents

Heat-conductive silicone gel composition

Info

Publication number
JP2001329173A
JP2001329173A JP2000154141A JP2000154141A JP2001329173A JP 2001329173 A JP2001329173 A JP 2001329173A JP 2000154141 A JP2000154141 A JP 2000154141A JP 2000154141 A JP2000154141 A JP 2000154141A JP 2001329173 A JP2001329173 A JP 2001329173A
Authority
JP
Japan
Prior art keywords
silicone gel
heat
thermally conductive
conductive filler
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2000154141A
Other languages
Japanese (ja)
Other versions
JP3531805B2 (en
Inventor
Hajime Funahashi
一 舟橋
Ikuko Miyamoto
育子 宮本
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fuji Polymer Industries Co Ltd
Original Assignee
Fuji Polymer Industries Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fuji Polymer Industries Co Ltd filed Critical Fuji Polymer Industries Co Ltd
Priority to JP2000154141A priority Critical patent/JP3531805B2/en
Publication of JP2001329173A publication Critical patent/JP2001329173A/en
Application granted granted Critical
Publication of JP3531805B2 publication Critical patent/JP3531805B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To obtain a heat-conductive silicone gel composition having improved peelability from a releasing paper mounting and between cut faces in the case of curing a compound composition containing a silicone gel and a heat- conductive filler. SOLUTION: The objective composition contains 100 pts.wt. of a silicone gel and 50-2,500 pts.wt. of a heat-conductive filler. The heat-conductive filler is surface-treated with at least one kind of silane coupling agent selected from isobutyltrimethoxysilane, isobutyltriethoxysilane, n-butyltrimethoxysilane and n-butyltriethoxysilane.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、難燃性及び電気絶
縁性を有する熱伝導性シリコーンゲル組成物に関するも
のであり、電子部品などの熱伝導部品、電気絶縁用部品
などとして適用される。さらに詳しくは離型台紙からの
剥離が良好なる熱伝導性シリコーンゲル組成物に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thermally conductive silicone gel composition having flame retardancy and electrical insulation, and is applied as a thermally conductive component such as an electronic component, a component for electrical insulation, and the like. More particularly, the present invention relates to a thermally conductive silicone gel composition which can be easily peeled from a release liner.

【0002】[0002]

【従来の技術】従来、トランジスタ、ダイオード,変圧
器,CPU,サイリスタなどの電子部品は使用中に発熱
し、その熱のため電子部品の性能が低下することがあ
る。そのため発熱するような電子部品には放熱体が取り
付けられる。これら発熱素子と放熱体の間には通常、イ
ンターフェイスとして放熱シートが用いられる。最近で
は、放熱シートとして熱伝導性シリコーンゲルがあり、
これらは非常に柔らかいため放熱体と発熱素子との密着
性がよいため盛んに使用されるようになってきた。
2. Description of the Related Art Conventionally, electronic components such as transistors, diodes, transformers, CPUs, and thyristors generate heat during use, and the performance of the electronic components may deteriorate due to the heat. Therefore, a heat radiator is attached to an electronic component that generates heat. Generally, a heat radiating sheet is used as an interface between the heat generating element and the heat radiating body. Recently, there is a heat conductive silicone gel as a heat dissipation sheet,
Since these are very soft, the adhesion between the heat radiator and the heat generating element is good, so that they have been widely used.

【0003】[0003]

【発明が解決しようとする課題】しかしながら最近は高
熱伝導性の放熱シートが求められることもあってシリコ
ーンゲルに添加する熱伝導性フィラーを大量に入れる必
要がある。ところが、シリコーンゲルに大量に熱伝導性
フィラーを添加するとコンパウンドの流動性がなくなり
加工しにくくなったりそのコンパウンドの硬化物は硬く
脆くなったりするという問題があった。
However, recently, a heat-radiating sheet having high heat conductivity has been demanded, and it is necessary to add a large amount of heat-conductive filler to be added to the silicone gel. However, when a large amount of the thermally conductive filler is added to the silicone gel, there is a problem that the compound loses fluidity and is difficult to process, and a cured product of the compound becomes hard and brittle.

【0004】これらを解決するために最近では特開20
00−1616号公報のように炭素数の多いシランカッ
プリング剤を使用してシリコーンゲルとの親和性を高め
ることで高充填する例がある。
In order to solve these problems, recently, Japanese Patent Laid-Open No.
As described in JP-A-00-1616, there is an example in which a silane coupling agent having a large number of carbon atoms is used to increase the affinity with a silicone gel to thereby achieve high filling.

【0005】しかしながら、炭素数の多いランカップリ
ング剤を使用するとそのコンパウンドの硬化物の表面が
べたつき離型台紙から製品を取り出しにくくなったり、
カット面同士がくっつくという問題があった。
However, when a run coupling agent having a large number of carbon atoms is used, the surface of the cured product of the compound becomes sticky and it becomes difficult to take out the product from the release liner.
There was a problem that the cut surfaces were stuck together.

【0006】本発明は、前記従来の課題を解決するた
め、シリコーンゲルへの熱伝導性フィラーの充填性をよ
くし、さらに硬化物が離型台紙からの剥がれが良好であ
ること同時にカット面同士の剥がれが良好である熱伝導
性シリコーンゲル組成物を提供することを目的とする。
[0006] In order to solve the above-mentioned conventional problems, the present invention improves the filling property of the thermally conductive filler into the silicone gel, and furthermore, the cured product has good peeling off from the release liner, and at the same time, the cut surfaces are separated from each other. It is an object of the present invention to provide a thermally conductive silicone gel composition which has good peeling.

【0007】[0007]

【課題を解決するための手段】前記目的を達成するた
め、本発明の熱伝導性シリコーンゲル組成物は、シリコ
ーンゲル:100重量部に対して熱伝導性フィラー50
〜2500重量部を含む組成のコンパウンドであって、
前記熱伝導性フィラーは、イソブチルトリメトキシシラ
ン,イソブチルトリエトキシシラン,n−ブチルトリメ
トキシシラン及びn−ブチルトリエトキシシランから選
択される少なくとも一つのシランカップリング剤で表面
処理されていることを特徴とする。
In order to achieve the above object, the thermally conductive silicone gel composition of the present invention comprises a silicone gel: 100 parts by weight and a thermally conductive filler 50 per 100 parts by weight.
A composition comprising 2500 parts by weight,
The thermal conductive filler is surface-treated with at least one silane coupling agent selected from isobutyltrimethoxysilane, isobutyltriethoxysilane, n-butyltrimethoxysilane, and n-butyltriethoxysilane. And

【0008】前記組成物においては、シランカップリン
グ剤は、熱伝導性フィラーに対して0.2〜10重量%
の範囲付与されていることが好ましい。
In the above composition, the silane coupling agent is contained in an amount of 0.2 to 10% by weight based on the heat conductive filler.
Is preferably provided.

【0009】また前記組成物においては、熱伝導性フィ
ラーが、酸化アルミニウム,酸化亜鉛,酸化マグネシウ
ム及び窒化硼素から選ばれる少なくとも一つの無機粒子
であることが好ましい。
In the above composition, it is preferable that the heat conductive filler is at least one inorganic particle selected from aluminum oxide, zinc oxide, magnesium oxide and boron nitride.

【0010】また前記組成物においては、熱伝導性フィ
ラーの平均粒子径が0.010〜10μmの範囲である
ことが好ましい。
[0010] In the composition, it is preferable that the average particle diameter of the thermally conductive filler is in the range of 0.010 to 10 µm.

【0011】本発明のコンパウンド組成物の硬化物は、
離型台紙からの剥がれが良好であること同時にカット面
同士の剥がれが良好である。
The cured product of the compound composition of the present invention comprises
The peeling from the release liner is good, and at the same time the peeling between the cut surfaces is good.

【0012】[0012]

【発明の実施の形態】シランカップリング剤はイソブチ
ルトリメトキシシラン,イソブチルトリエトキシシラ
ン,n−ブチルトリメトキシシラン,n−ブチルトリエ
トキシシランから選択されるものでシリコン元素に直接
結合するアルキル基の炭素数が4個のものが好ましい。
DESCRIPTION OF THE PREFERRED EMBODIMENTS A silane coupling agent is selected from isobutyltrimethoxysilane, isobutyltriethoxysilane, n-butyltrimethoxysilane, and n-butyltriethoxysilane, and is used for forming an alkyl group directly bonded to a silicon element. Those having 4 carbon atoms are preferred.

【0013】表面処理の方法はすでに公知となっている
乾式法,湿式法,インテグラル法などがあり、どれを用
いてもよい。
The method of surface treatment includes a well-known dry method, wet method, integral method and the like, and any of them may be used.

【0014】離型台紙はポリエステル,ポリイミド,ポ
リオレフィン,フッ素フィルムから選択することが好ま
しい。離型効果を高めるためこれらのフィルム表面には
フッ素化合物,シリコーン化合物,アクリル樹脂,メラ
ミン樹脂を塗布してもよい。また、制電処理,ブラスト
処理をしたフイルムを使用してもよい。
Preferably, the release liner is selected from polyester, polyimide, polyolefin, and fluorine film. These films may be coated with a fluorine compound, a silicone compound, an acrylic resin, or a melamine resin to enhance the release effect. Further, a film which has been subjected to antistatic processing and blast processing may be used.

【0015】本発明には、難燃性付与のため白金系化合
物を添加しもよい。白金系化合物としては塩化白金酸,
アルコール変性塩化白金,白金オレフィン錯体,メチル
ビニルポリシロキサン白金錯体から選ばれる少なくとも
ひとつであることが好ましい。
In the present invention, a platinum compound may be added for imparting flame retardancy. Platinum compounds include chloroplatinic acid,
It is preferably at least one selected from alcohol-modified platinum chloride, a platinum olefin complex, and a methylvinylpolysiloxane platinum complex.

【0016】また、難燃助剤として酸化鉄,酸化チタ
ン,水酸化アルミニウム,水酸化マグネシウムなどがあ
り一種または二種の混合物が好適に用いられる。
As the flame retardant aid, there are iron oxide, titanium oxide, aluminum hydroxide, magnesium hydroxide and the like, and one or two kinds of mixtures are suitably used.

【0017】前記した、本発明の熱伝導性シリコーンゲ
ル組成物はシリコーンゲル100重量部に対してイソブ
チルトリメトキシシラン,イソブチルトリエトキシシラ
ン,n−ブチルトリメトキシシラン,n−ブチルトリエ
トキシシランから選択されるシランカップリング剤で表
面処理をした熱伝導性フィラー50〜2500重量部か
らなる組成コンパウンドでありその硬化物が離型台紙か
らの剥がれが良好であることと同時にカット面同士の剥
がれが良好である熱伝導性シリコーンゲル組成物とな
る。
The heat conductive silicone gel composition of the present invention is selected from isobutyltrimethoxysilane, isobutyltriethoxysilane, n-butyltrimethoxysilane, and n-butyltriethoxysilane per 100 parts by weight of the silicone gel. It is a composition compound consisting of 50 to 2500 parts by weight of a thermally conductive filler surface-treated with a silane coupling agent to be cured. The cured product has good peeling from the release liner and good peeling between cut surfaces. And a thermally conductive silicone gel composition.

【0018】[0018]

【実施例】以下実施例により本発明をさらに具体的に説
明する。
The present invention will be described more specifically with reference to the following examples.

【0019】酸化アルミニウムは昭和電工(株)製AS
−30(平均粒径 17μm)を使用した。酸化アルミ
ニウムはフィラーの1.0重量%のシランカップリング
剤ですべて乾式法によって処理した。離型台紙はポリプ
ロピレンフィルムを使用した。
Aluminum oxide is manufactured by Showa Denko KK AS
-30 (average particle size: 17 μm) was used. The aluminum oxide was all treated by a dry method with a silane coupling agent of 1.0% by weight of the filler. The release liner used a polypropylene film.

【0020】[0020]

【実施例1】シリコーンゲル100重量部(JCR61
06 東レ・ダウコーニングシリコーン(株)製)にイ
ソブチルトリメトキシシランで処理をした酸化アルミニ
ウムを800重量部を添加して混練りすることによって
液状のコンパウンドを得た。これをプレス成型すること
でシートを得ることができた。
Example 1 100 parts by weight of silicone gel (JCR61)
06 Toray Dow Corning Silicone Co., Ltd.) was mixed with 800 parts by weight of aluminum oxide treated with isobutyltrimethoxysilane and kneaded to obtain a liquid compound. This was press-molded to obtain a sheet.

【0021】[0021]

【実施例2】シリコーンゲル100重量部(JCR61
06 東レ・ダウコーニングシリコーン(株)製)にn
−ブチルトリメトキシシランで処理をした酸化アルミニ
ウムを800重量部を添加して混練りすることによって
液状のコンパウンドを得た。これをプレス成型すること
でシートを得ることができた。
Example 2 100 parts by weight of silicone gel (JCR61)
06 Toray Dow Corning Silicone Co., Ltd.)
A liquid compound was obtained by adding and kneading 800 parts by weight of aluminum oxide treated with -butyltrimethoxysilane. This was press-molded to obtain a sheet.

【0022】[0022]

【比較例1】シリコーンゲル100重量部(JCR61
06 東レ・ダウコーニングシリコーン(株)製)にメ
チルトリメトキシシランで処理をした酸化アルミニウム
を800重量部を添加して混練りすることによって液状
のコンパウンドを得た。これをプレス成型することでシ
ートを得ることができた。
Comparative Example 1 100 parts by weight of silicone gel (JCR61)
06 Toray Dow Corning Silicone Co., Ltd.) was mixed with 800 parts by weight of aluminum oxide treated with methyltrimethoxysilane and kneaded to obtain a liquid compound. This was press-molded to obtain a sheet.

【0023】[0023]

【比較例2】シリコーンゲル100重量部(JCR61
06 東レ・ダウコーニングシリコーン(株)製)にn
−ヘキシルトリメトキシシランで処理をした酸化アルミ
ニウムを800重量部を添加して混練りすることによっ
て液状のコンパウンドを得た。これをプレス成型するこ
とでシートを得ることができた。
Comparative Example 2 100 parts by weight of silicone gel (JCR61)
06 Toray Dow Corning Silicone Co., Ltd.)
A liquid compound was obtained by adding and mixing 800 parts by weight of aluminum oxide treated with hexyltrimethoxysilane. This was press-molded to obtain a sheet.

【0024】[0024]

【比較例3】シリコーンゲル100重量部(JCR61
06 東レ・ダウコーニングシリコーン(株)製)にn
−オクチルトリメトキシシランで処理をした酸化アルミ
ニウムを800重量部を添加して混練りすることによっ
て液状のコンパウンドを得た。これをプレス成型するこ
とでシートを得ることができた。
Comparative Example 3 100 parts by weight of silicone gel (JCR61)
06 Toray Dow Corning Silicone Co., Ltd.)
A liquid compound was obtained by adding and kneading 800 parts by weight of aluminum oxide treated with octyltrimethoxysilane. This was press-molded to obtain a sheet.

【0025】[0025]

【比較例4】シリコーンゲル100重量部(JCR61
06 東レ・ダウコーニングシリコーン(株)製)にn
−ドデシルトリメエトキシシランで処理をした酸化アル
ミニウムを800重量部を添加して混練りすることによ
って液状のコンパウンドを得た。これをプレス成型する
ことでシートを得ることができた。
Comparative Example 4 100 parts by weight of silicone gel (JCR61)
06 Toray Dow Corning Silicone Co., Ltd.)
-A liquid compound was obtained by adding and mixing 800 parts by weight of aluminum oxide treated with dodecyltrimethyoxysilane. This was press-molded to obtain a sheet.

【0026】[0026]

【比較例5】シリコーンゲル100重量部(JCR61
06 東レ・ダウコーニングシリコーン(株)製)にn
−ヘキサデシルトリメトキシシランで処理をした酸化ア
ルミニウムを800重量部を添加して混練りすることに
よって液状のコンパウンドを得た。これをプレス成型す
ることでシートを得ることができた。
Comparative Example 5 100 parts by weight of silicone gel (JCR61)
06 Toray Dow Corning Silicone Co., Ltd.)
-A liquid compound was obtained by adding and mixing 800 parts by weight of aluminum oxide treated with hexadecyltrimethoxysilane. This was press-molded to obtain a sheet.

【0027】シリコーン元素に直接結合したアルキル基
の炭素数と化学式とともに硬度,フィルムとの剥離力,
カット面の状態結果を以下に示す。
The hardness, peeling strength with the film, the number of carbon atoms and the chemical formula of the alkyl group directly bonded to the silicone element,
The state results of the cut surface are shown below.

【0028】[0028]

【表1】 [Table 1]

【0029】硬度はアスカーC硬度計で測定した。剥離
力はJIS Z 0237を参照にして測定した。(測
定サンプル幅50mm) カット面の状態はプレス成型したシートを任意の大きさ
にカットし2週間室温で放置した。2週間室温で放置し
たのち離型台紙からカットした製品を取り出すときに取
り出す製品の隣にある製品が追従するかしないかで判定
し追従しなかったら良好とした。
The hardness was measured with an Asker C hardness tester. The peeling force was measured with reference to JIS Z0237. (Measurement sample width: 50 mm) As for the state of the cut surface, a press-formed sheet was cut into an arbitrary size and left at room temperature for 2 weeks. After leaving the product at room temperature for 2 weeks, when removing the cut product from the release liner, it was determined whether or not the product next to the product to be removed followed or not.

【0030】前記表1に示すとおり、比較例1はシリコ
ーン元素に直接結合したアルキル基の炭素数が1個の場
合でありシリコーンゲルとの親和性が低いため硬度は高
くかつ充填性が悪い。逆にフィルムからの剥離性または
カット面同士はくっつくことなく良好であった。
As shown in Table 1 above, Comparative Example 1 is a case where the alkyl group directly bonded to the silicone element has one carbon atom, and has a low affinity with the silicone gel, so that the hardness is high and the filling property is poor. Conversely, the releasability from the film or the cut surfaces were good without sticking.

【0031】比較例2〜5はシリコーン元素に直接結合
したアルキル基の炭素数が6個以上の場合であり炭素数
が多いほどシリコーンゲルとの親和性が高いため硬度は
低くかつ充填性が良好である。逆に炭素数が多いシラン
カップリング剤を使用すると硬化物はべたつく傾向にな
るためフィルムからの剥離性は悪くなりさらに、カット
面同士はくっつき硬化物を離型台紙から取り出すときは
甚だ困難であった。
In Comparative Examples 2 to 5, the number of carbon atoms of the alkyl group directly bonded to the silicone element is 6 or more. The higher the number of carbon atoms, the higher the affinity for the silicone gel, and the lower the hardness and the better the filling property. It is. Conversely, when a silane coupling agent having a large number of carbon atoms is used, the cured product tends to be sticky, so that the releasability from the film is deteriorated. Was.

【0032】ところが、シリコーン元素に直接結合した
アルキル基の炭素数が4個の場合はシリコーンゲルとの
親和性は程々であるため硬度,充填性,剥離性,カット
面同士の状態は良好であった。
However, when the number of carbon atoms in the alkyl group directly bonded to the silicone element is four, the affinity with the silicone gel is moderate, so that the hardness, the filling property, the releasability, and the state of the cut surfaces are good. Was.

【0033】[0033]

【発明の効果】以上説明したとおり、本発明によればシ
リコーンゲル100重量部に対してイソブチルトリメト
キシシラン,イソブチルトリエトキシシラン,n−ブチ
ルトリメトキシシラン,n−ブチルトリエトキシシラン
から選択されるシランカップリング剤で表面処理をした
熱伝導性フィラー50〜2500重量部からなる組成コ
ンパウンドでありその硬化物は離型台紙からの剥がれが
良好であることと同時にカット面同士の剥がれが良好で
ある熱伝導性シリコーンゲル組成物を得ることができ
る。
As described above, according to the present invention, isobutyltrimethoxysilane, isobutyltriethoxysilane, n-butyltrimethoxysilane, and n-butyltriethoxysilane are selected from 100 parts by weight of the silicone gel. A composition compound consisting of 50 to 2500 parts by weight of a thermally conductive filler surface-treated with a silane coupling agent. The cured product has good peeling from the release liner and good peeling between cut surfaces. A thermally conductive silicone gel composition can be obtained.

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】シリコーンゲル:100重量部に対して熱
伝導性フィラー50〜2500重量部を含む組成のコン
パウンドであって、前記熱伝導性フィラーは、イソブチ
ルトリメトキシシラン,イソブチルトリエトキシシラ
ン,n−ブチルトリメトキシシラン及びn−ブチルトリ
エトキシシランから選択される少なくとも一つのシラン
カップリング剤で表面処理されていることを特徴とする
熱伝導性シリコーンゲル組成物。
1. Silicone gel: a compound having a composition containing 50 to 2500 parts by weight of a thermally conductive filler with respect to 100 parts by weight, wherein the thermally conductive filler is composed of isobutyltrimethoxysilane, isobutyltriethoxysilane, n A thermally conductive silicone gel composition, which is surface-treated with at least one silane coupling agent selected from -butyltrimethoxysilane and n-butyltriethoxysilane.
【請求項2】シランカップリング剤が、熱伝導性フィラ
ーに対して0.2〜10重量%の範囲付与されている請
求項1に記載の熱伝導性シリコーンゲル組成物。
2. The thermally conductive silicone gel composition according to claim 1, wherein the silane coupling agent is provided in a range of 0.2 to 10% by weight based on the thermally conductive filler.
【請求項3】熱伝導性フィラーが、酸化アルミニウム,
酸化亜鉛,酸化マグネシウム及び窒化硼素から選ばれる
少なくとも一つの無機粒子である請求項1に記載の熱伝
導性シリコーンゲル組成物。
3. The method according to claim 1, wherein the thermally conductive filler is aluminum oxide,
The thermally conductive silicone gel composition according to claim 1, wherein the composition is at least one inorganic particle selected from zinc oxide, magnesium oxide, and boron nitride.
【請求項4】熱伝導性フィラーの平均粒子径が0.01
0〜100μmの範囲である請求項1に記載の熱伝導性
シリコーンゲル組成物。
4. The heat conductive filler has an average particle diameter of 0.01.
The thermally conductive silicone gel composition according to claim 1, which is in a range of 0 to 100 µm.
JP2000154141A 2000-05-25 2000-05-25 Sheet containing thermal conductive silicone gel Expired - Lifetime JP3531805B2 (en)

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JP2010539668A (en) * 2007-09-20 2010-12-16 アーベーベー・リサーチ・リミテッド Electrically insulated device and electrical device provided with the same
CN108384246A (en) * 2018-04-09 2018-08-10 王景硕 A kind of preparation method of addition thermal conductive Silica hydrogel
CN111286200A (en) * 2018-12-06 2020-06-16 北京化工大学 High-softness low-exudation heat-conducting silicone gel and preparation method thereof

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CN111286200B (en) * 2018-12-06 2021-06-08 北京化工大学 High-softness low-exudation heat-conducting silicone gel and preparation method thereof

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